Process of making margarine



Patented Dec. 25, 1934 I UNITED STATES PATENT OFFICE raoosss or m: I I CBenjamin 1:. Harris, Chicago,

No Drawing.

11 Claims. 1 (Cl. 99-13) My invention relates to the manufacture ofmargarine and is a continuation in part of my copending applicationSerial No. 697,534, filed November 8, 1933. My present invention is alsoa continuation in part of my prior application,

Serial #685,081, filed August 14, 1933.

My prior application, of which the present is a division, describes theformation of new chemical substances adapted for use in emulsionsgenerally and whenever interface modifying properties are desired. Thematerial there described is particularly advantageous, however, in theproduction of margarine. As described, in some detail in my prior PatentNo. 1,917,254, conventional margarine suffers from so-called weeping orleaking of the moisture therefrom. In my prior patent, I disclose amethod of preventing thisleaking or weeping action by the use ofmaterials of a class I. term hydrophyllic lipins. The chemicalcomposition described in application Serial No. 697,534 referred toabove may be termed a hydrophylllo lipin and possesses thecharacteristics of the materials described in the prior patent.

The principal object of the present invention is the use in margarine ofmaterials of the class described in my copending application.

Another object is the provision of an improved method of producing anon-weeping margarine.

Other objects and features of the invention will be apparent as thedescription progresses.

Those skilled in the art are referred to my copending application for acomplete description of the manner of making the materials of myinvention. In general, the method comprises treatment of an ordinarytriglyceride, such as the oils and fats of commerce, to produce thereina proportion of various fatty acid diglycerides and usually lesserproportions of mixtures of various fatty acid mono-glycerides havingfree hydroxy' groups. The composition as a whole has definitehydrophillic properties and is capable of dispersing in aqueous media,producing pastes of varying moisture concentration which lend themselvesto dispersion in plastic margarine. This hydrophillic material, whenemployed in margarine, will prevent weeping thereof and assist inmaintaining a more stable emulsion. These materials are preferablyproduced in the form of an aqueous paste and in this form, either withor without the use of additional moisture, are blended into thecompleted plastic margarine emulsion.

There are essentially three steps inthe production ,of the margarineaccording to my invention,

namely, the formation of the plastic margarine emulsion; the formationof. the hydrophillic material, preferably as dispersed in aqueous media,in paste, or other form; and the blending of this paste with or withoutadditionalmoisture into the plastic margarine mass. In order that thepresent disclosure may be complete,'I shall first describe the method ofmaking my improved hydrophillic materials.

The'g'eneral process comprises partially saponifying a triglyceride withan alkaline saponifying. agent, the quantity of alkali employed beinginsuflicient to completely saponify the triglyceride. The resultingmixture contains a plurality of fatty acid esters with free hydroxygroups with some soap. The soap in the mixture is then decomposed eitherin whole or in part with an acid. When the material is employed inmargarine, an innocuous acid should be selected such as hydrochloricacid, phosphoric acid, tartaric acid, lactic acid, citric acid. and thelike. The alkaline saponifying agent is preferably introduced melted butmay be introduced in other forms into the triglyceride, and the reactionallowed to proceed at a suitable temperature. In my preferred man- .nerof carrying out the process, the partially saponifled mixture isemulsified with approximately its own weight of water'to form a paste.This paste is then treated with the acid to decompose the soap thereineither in whole or in part. The following examples are illustrative ofthe manner of preparing the hydrophyllic material.

Example No. 1

500 parts of hydrogenated cottonseed oil (melting point 140? F.) aremelted and kept at a temperature-of 220C. To this is added,withstirring, a eutectic mixture of 12 parts of caustic soda and 17%parts of caustic potash,'also melted and kept at 220 C. Vigorousstirrihg is continued for ten minutes.

This molten mixture is then cooled to about 170 C. and poured gradually,with stirring, 'into 500 parts of water at C. The paste is then cooleddown to about 40 0., when 47.5 parts of "concentr'ated hydrochloricacid, diluted with parts of water, are stirred in. The resultant productis apaste' which lends itself readily to incorporation witholeomargarlne in a margarine blender. n

- 4 Example No. 2 Y

500 parts of partially hydrogenated cottonseed oil (melting point aboutF.) are melted and kept at a temperature of 3P0 to 235 C. To this isadded, with stirring, a eutectic mixture of 12 parts of caustic soda and17 parts of caustic potash, also melted and kept at 220 to 235 C.Vigorous stirring is continued for ten minutes.

This molten mixture is then cooled to about 170 C. and poured gradually,with stirring, into 500 parts of water at 70 C. The paste is then cooleddown to about 40 C., when 62.5 parts of concentrated hydrochloric acid,diluted with 90 parts of water, are stirred in. The resultant product isa paste which lends itself readily to incorporation with oleomargarinein a margarine blender.

The present example differs from Example 1 in that the paste issubstantially completely neutralized. With the percentages of materialsgiven, the resulting product is approximately neutral to litmus.

Example No. 3

400 parts of oleostearine are melted, heated and kept at 200 C. To thismelt are added, with vigorous stirring, 20 parts of caustic sodadissolved in 30 parts of water. The caustic soda solution is added veryslowly at first so as to keep the foaming down to a minimum. As the foamgradually subsides, more caustic soda solution is added. During theaddition of the caustic solution, the temperature of the oleostearinedrops to about 180 C. and is maintained at this temperature by supplyingsuflicient heat to the melt.

After all the caustic soda is in, the stirring is continued for anadditional five to ten minutes. This melt is then run, with agitation,into 400 parts of water at C. This mixture is then heated andsimultaneously stirred until a smooth, dispersed product is obtained.This is cooled down to 30 C. and 130 parts of 28% lactic acid arestirred in.

The product is a homogeneous paste with marked water-imbibing propertiesand readily blendable with margarine.

Example No. 4

300 parts of cottonseed stearine (iodine number not over 90) are meltedto 175 C. and treated with 15 parts of caustic soda dissolved in 65parts of glycerol, and heated to the same temperature. The glycerol-sodasolution is added gradually with stirring and heat control so that atemperature of approximately 175 is maintained throughout. There is somefoaming, but not very much.

After all the glycerol-soda is in, the heating and stirring arecontinued for an additional five minutes. This mixture is then run into300 parts of water kept at 70 C. and stirring is continued until asmoothly dispersed paste is obtained and the temperature has dropped toabout 45 C. Finally, into this paste are mixed 62 parts of aqueoushydrochloric acid, 20% solution.

Example No. 5

400 parts of oleostearine are melted, heated and kept at 200 C. To thismelt are added, with vigorous stirring, 20 parts of caustic sodadissolved in 30 parts of water. The caustic soda solution is added veryslowly at first so as to keep the foaming down to a As the foamgradually subsides, more caustic soda solution is added. During theaddition of the caustic solution, the temperature of the oleostearinedrops to about 180 C. and is maintained at this temperature by supplyingsufiicient heat to the melt.

After all the caustic soda is in, the stirring is continued for anadditional five to ten minutes. This melt is then run, with agitation,into 400 parts of water at 75 C. This mixture is then heated andsimultaneously stirred until a smooth dispersed product is obtained.This is cooled down to 30 C. and 161 parts of 28% lactic acid arestirred in.

The paste so produced may be diluted to contain 75 to of moisture, and,although it contains a large proportion of diglycerides, it is easilyblended into plastic margarine.

More than the above stated PrODOI'tiOIIS of kali may be used, in whichcase less unchanged triglyceride will appear in the final product underthe above prescribed conditions. If desired, however, smallerproportions of alkali than those indicated may be used, in which casethe product will contain a lesser proportion of modified triglyceridethan in the above examples, and a greater proportion of unchangedtriglyceride. The proportion of acid also may be varied a great deal,depending upon the characteristics desired in the final product,Obviously the hydrogen ion concentration and/ or the amount of soappresent will be determined by the amount of acid used. The larger theamount of acid used, the greater will be the proportion of free fattyacids, and less soap in the finished product.

If suflicient acid is used to neutralize the reaction mixture as, forinstance, in Example No. 5, the resulting reaction product will form asmooth paste which can be incorporated in plastic margarine and afiectthe interfaces of the emulsion sufficiently to make the margarinenonleaking and keep the desired amount of moisture therein. However, aslight amount of soap may remain if desired, such as, for example, about1% or less, or, as in some of the examples, if about 75 to of the soapis neutralized, based on the amount of alkali employed.

In the preferred manner of use, the paste is made prior toneutralization thereof, in which case, even though it is madesubstantially neutral, as described in Example 5, it will remain smooth,can be thinned out with additional amounts of aqueous material, and isreadily blended into the margarine where it will perform its role instabilizing the emulsion and drying up interstitial moisture.

In incorporating the paste into the margarine, the latter is madeaccording to any suitable formula and processed to the plastic emulsionstage where it is ready for treatment on a blender. Assume the paste isof the 50% character, that is with equal amounts of water andhydrophilic material. In order to incorporate this paste better into themargarine, about an equal amount of moisture is added, leaving the pastewith about 20 to 25% of solid material. This paste may be still furtherdiluted, if desired.

In the blending operation, lbs. of the plas-.- tic margarine are placedin a blender, preferably with 2 type agitators and 2% of the 25% pasteadded. This represents about of the hydrophyllic material made inaccordance with the ex-- amples given. Additional milk may also beplaced in the blender together with salt and sodium benzoate, and theblender operated until all moisture is taken up and the product ishomogeneous. In

the example given, a dry homogeneous margarine is easily produced with amoisture content ranging from 16% to 17%. Although the hydrophyllicmaterial of my invention may contain a large amount of diglycerides, itis readily incorporated into the plastic margarine, even thoughordinarily a diglyceride is incorporated into margarine usually withsome difliculty. This ease of incorporation seems to be due to the factthat the digylcerides of my hydrophillic material are interspersed withother media which facilitate and enhance its dispersibility in theplastic margarine.

In the margarine blending operation described hereinabove, the amount ofmy hydrophyllic material employed is based upon dry weights. This is notto be taken as a limitation of the amount to be used,'since as little as/4% of the hydrophyllic material produces a marked effect in a margarinewith approximately 16 to 17% of moisture. Approximately twice thisamount produces a more marked effect, and even somewhat greater amountsmay be employed should it be desired to incorporate a still largeramount of moisture in the margarine. However, the amount should not behigh enough to change the physical characteristics of the margarine,such as texture,

grain and palatability. It is to be noted that the amount of moistureretained in the margarine by the material of my invention is notexplained by the absorption thereof by the hydrophyllic lipin itself, asthe amount used is very small. It is due rather to the interfacemodifyingcharacteristics of the hydrophyllic lipin whereby the water isbound at the interfaces even though it may not have been completelyemulsified in the original emulsion.

What I claim as new and desire to protect by Letters Patent of theUnited States is: I

1. The method of making an improved margarrine, which comprises forminga plastic margarine emulsion of oleaginous and aqueous materials,partially saponifying an oleaginous material of a class consisting ofoils and fats, forming an aqueous paste of the resulting product,neutralizing said paste, and blending the paste into the plasticmargarine emulsion.

2. The method of making an improved margarine, which comprises forming aplastic margarine emulsion of oleaginous and aqueous materials,partially saponifying. an oleaginous material of a class consisting ofoils and fats, forming an aqueous paste of the resulting product,neutralizing said paste, and blending the paste with an additionalamount of aqueous material into the plastic margarine emulsion.

3. The method of making an improved margarine, which comprises forming aplastic margarine emulsion of oleaginous and aqueous materials,partially saponifying an oleaginous material of a class consisting ofoils and fats, forming an aqueous paste of the resulting product,neutralizing said paste, and blending the paste into the plasticmargarine emulsion together with an accessory substance of a classconsisting of salt and benzoate.

4. The method of making an improved margarine which comprises forming aplastic margarine emulsion, adding to a material of a class consistingof oils and fats. a proportion of an alkali sufficient to partiallysaponify such material, heating the mixture to reaction, forming anaqueous paste of the resulting material, and blending said paste intothe plastic margarine emulsion.

5. The method of making an improved margarine which comprises forming aplastic margarine emulsion, adding to a material of a class consistingof oils and fats, a proportion of an alkali sufficient to partiallysaponify such material, heating the mixture to reaction; forming anaqueous paste of the resulting material, neutralizing said paste, andblending said paste into the plastic margarine emulsion.

6. The method of making an improved margarine which comprises forming aplastic margarine emulsion, adding to a material of a class consist-,

ing of oils and fats, a proportion of an alkali sufficient to partiallysaponify such material, heating the mixture to reaction, forming anaqueous paste of the resulting material, neutralizing said paste, addingan additional amount of aqueous liquid thereto to thin the same, andblending the thinned paste into the plastic margarine emulsion.

7. The method of making an improved margarine which comprises forming aplastic margarine emulsion, partially saponifying a hydrogenated liquidoil, forming an aqueous paste of the partially saponified oil,neutralizing the same, and blending the neutralized paste into theplastic margarine emulsion.

8. The method of making an improved margarine which comprises forming aplastic margarine emulsion, partially saponifying a hydrogenatedcottonseed oil, forming an aqueous paste of the partially saponi'fiedoil, neutralizing the same, and blending the neutralized paste into theplastic margarine emulsion.

9. The methodof making an improved margarine, which comprises forming aplastic margarine emulsion, partially saponifying a hydrogenatedoleostearine, forming an aqueous paste of the partially saponified oil,neutralizing the same, and blending the neutralized paste into theplastic margarine emulsion.

10. The method of making an improved margarine which includes the stepof blending into said margarine while in a plastic form a hydrophyllicmaterial in paste form formed by partially saponifying an oleaginousmaterial of a class consisting of oils and fats, and neutralizing thepartially saponified product to form a mixture including a proportion offatty acid, monoand di-glycerides.

11. An improved substantially dry margarine comprising a plasticemulsion of oleaginous and aqueous materials, and. a relatively smallamount of the product of the partial saponification of a triglycerideoil or fat and the neutralization thereof, said product containing amixture of mono and diglycerides and a substantial amount of free fattyacids.

BENJAMIN R. HARRIS.

